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探讨使用软木颗粒在酒吧吸附微萃取中的应用,以气相色谱/电子捕获检测定量法测定水样中的有机氯农药。

Exploring the use of cork pellets in bar adsorptive microextraction for the determination of organochloride pesticides in water samples with gas chromatography/electron capture detection quantification.

机构信息

Universidade Federal de Santa Catarina (UFSC), Departamento de Química, Florianópolis, SC 88040-900, Brazil.

Universidade Federal de Santa Catarina (UFSC), Departamento de Química, Florianópolis, SC 88040-900, Brazil.

出版信息

J Chromatogr A. 2021 May 24;1645:462099. doi: 10.1016/j.chroma.2021.462099. Epub 2021 Mar 26.

Abstract

In this study, a biosorbent material with characteristics for the adsorption of organic compounds was used for a cork pellet-based bar adsorptive microextraction technique, as a new greener alternative for the determination of organochlorine compounds. Aldrin, chlordane, dieldrin, endrin, lindane, 4,4-DDD, 4,4-DDE, 4,4-DDT, α-endosulfan and β-endosulfan were analyzed in water samples (drinking water, stream water and river water) with separation/detection by gas chromatography and electron capture detection (GC/ECD). The parameters that can affect the sample preparation efficiency such as desorption solvent and time as well as extraction time and ionic strength were evaluated by multivariate and univariate designs. Cork pellets (10  ×  Ø 3 mm) were used for the extraction of 15 mL of sample in the optimal conditions: 60 min of agitation with no salt added to the sample, followed by desorption of the cork pellet with 120 µL of ethyl acetate for 30 min. The bar-to-bar RSD out with five different bars showed good results with RSD ≤ 15.6%, allowing the use of simultaneous extractions. LOD and LOQ values ranged from 3 to 15 ng L and 10 to 50 ng L respectively, and the determination coefficients were greater than 0.9869. The target analytes were not detected in the three analyzed samples. Therefore, the recovery study was performed fortifying the water samples. Analyte recovery ranged from 48.7 - 138.2% for drinking water, 40.2 - 128.2% for stream water and 67.5 - 128.7% for river water.

摘要

在这项研究中,使用具有吸附有机化合物特性的生物吸附材料,用于基于软木颗粒的棒状吸附微萃取技术,作为一种新的更环保的替代方法,用于测定有机氯化合物。水样(饮用水、溪水和河水)中的艾氏剂、氯丹、狄氏剂、异狄氏剂、林丹、4,4-DDD、4,4-DDE、4,4-DDT、α-硫丹和β-硫丹采用气相色谱和电子俘获检测(GC/ECD)进行分离/检测。通过多元和单因素设计评估了影响样品制备效率的参数,如解吸溶剂和时间以及萃取时间和离子强度。在最佳条件下,用 10ר3mm 的软木颗粒萃取 15mL 样品:在不向样品中加盐的情况下搅拌 60min,然后用 120µL 乙酸乙酯解吸软木颗粒 30min。在五个不同的棒之间进行的棒间 RSD 表现出良好的结果,RSD≤15.6%,允许同时进行萃取。LOD 和 LOQ 值范围分别为 3-15ng/L 和 10-50ng/L,测定系数大于 0.9869。在所分析的三个样品中均未检测到目标分析物。因此,进行了加标回收率研究。对于饮用水,回收率范围为 48.7-138.2%;对于溪水,回收率范围为 40.2-128.2%;对于河水,回收率范围为 67.5-128.7%。

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